CN113004119A - Preparation method of electronic-grade reagent - Google Patents
Preparation method of electronic-grade reagent Download PDFInfo
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- CN113004119A CN113004119A CN201911319061.3A CN201911319061A CN113004119A CN 113004119 A CN113004119 A CN 113004119A CN 201911319061 A CN201911319061 A CN 201911319061A CN 113004119 A CN113004119 A CN 113004119A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/94—Use of additives, e.g. for stabilisation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C315/00—Preparation of sulfones; Preparation of sulfoxides
- C07C315/06—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D231/00—Heterocyclic compounds containing 1,2-diazole or hydrogenated 1,2-diazole rings
- C07D231/02—Heterocyclic compounds containing 1,2-diazole or hydrogenated 1,2-diazole rings not condensed with other rings
- C07D231/10—Heterocyclic compounds containing 1,2-diazole or hydrogenated 1,2-diazole rings not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D249/00—Heterocyclic compounds containing five-membered rings having three nitrogen atoms as the only ring hetero atoms
- C07D249/16—Heterocyclic compounds containing five-membered rings having three nitrogen atoms as the only ring hetero atoms condensed with carbocyclic rings or ring systems
- C07D249/18—Benzotriazoles
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Abstract
The invention provides a preparation method of an electronic grade reagent, which comprises the following steps: adding raw materials to be purified and metal compounds into a rectification system for rectification; collecting the product after removing the former component; and detecting the content of metal ions and anions in the collected product to verify whether the purity of the product reaches the standard of the electronic grade reagent. According to the invention, a proper amount of metal compound is added during rectification, so that metal ions and anions can be reduced to ppb level in one step, especially the content of anions in the electronic-grade reagent is effectively reduced, the purity of the electronic-grade reagent is obviously improved, and the method has the advantages of simple steps, high purity and wider application range.
Description
Technical Field
The invention relates to a preparation method of an electronic grade reagent.
Background
The chemical reagents are divided according to the purity (the content of impurities), and the total number of the chemical reagents is 7, namely high purity, spectral purity, standard, spectral purity, superior purity, analytical purity, chemical purity and the like. The national and competent departments promulgate 3 types of main superior purity, graded purity and chemical purity of quality indexes. (1) The reagent has the highest purity, namely 99.8 percent of first-grade product or guaranteed reagent, has the lowest impurity content, is suitable for important and precise analysis work and scientific research work, and uses green bottle labels. (2) The purity of the analytical reagent, also called secondary reagent, is very high, 99.7%, is slightly inferior to the superior purity, and is suitable for important analysis and general research work, and a red bottle label is used. (3) The chemical purity, also called tertiary reagent, is more than or equal to 99.5 percent, has larger difference with the analytical purity, and is suitable for general analytical work of industrial, mining and school. Blue (dark blue) labels are used. (4) The test reagent is also called quaternary reagent. The reagent with purity much higher than the superior grade is called high-purity reagent (more than or equal to 99.99%). Highly pure reagents have been developed on the basis of general-purpose reagents, which are the reagents of the highest purity produced by special methods for the specific purpose of use. The high purity reagent is an electronic grade reagent if it is specific to a high purity chemical specific to optics and electronics.
The content of impurities in the electronic-grade reagent directly influences the electrical property and the yield of the integrated circuit, along with the rapid development of the integrated circuit, the distance between components is smaller and smaller, and trace impurities can cause the short circuit of a semiconductor device, so that higher and higher requirements are put forward on the electronic-grade reagent. The purity and cleanliness of the electronic-grade reagent have very important influences on the finished product rate, the electrical property, the reliability and the like.
Conventional electronic grade reagents can be obtained by rectification, which is a separation process that separates components by utilizing different volatility of the components in a mixture, and common equipment comprises a plate-type rectifying tower and a packing rectifying tower. The rectification is usually carried out in a rectification column, and gas and liquid phases are contacted in a countercurrent manner to carry out interphase heat and mass transfer. The volatile component in the liquid phase enters the gas phase, and the non-volatile component in the gas phase is transferred into the liquid phase, so that the nearly pure volatile component can be obtained at the top of the tower, and the nearly pure non-volatile component can be obtained at the bottom of the tower. Condensing the vapor led out from the tower top, returning a part of condensate as reflux liquid from the tower top to the rectifying tower, and obtaining the rest distillate as a tower top product. The liquid extracted from the tower bottom is partially gasified by a reboiler, the vapor rises along the tower, and the rest liquid is used as a tower bottom product. According to the steps of molecular sieve dehydration, resin dehydration, reverse osmosis, high-temperature rectification, ion exchange and circulating filtration, as shown in 102898275A, isopropanol with each metal ion concentration of less than 10ppt and each single anion concentration of less than 1ppb can be finally obtained. CN109251143A states, food grade ethyl lactate is used as raw material, through ion exchange resin adsorption, rectification and sub-boiling distillation, the metal ion content is less than 1ppb, and the acidity is less than 65 ppm.
Above we can find that rectification is an effective method for removing metal ions, but has limited effect on residual acids, and anions such as mineral acid groups (chloride, sulphate, nitrate) are difficult to remove completely by rectification, partly because they have a certain volatility and can be distilled off together with the material to be purified. If the material to be purified has a certain alkalinity, inorganic acid is often reacted with the material, such as compounds such as pyrazole and imidazole and hydrochloric acid can generate hydrochloride, and the hydrochloride can be distilled off together in the rectification process, thereby further increasing the difficulty of purification.
Therefore, the resin is often used in conjunction with rectification, cation exchange resin further removes metal ions, anion exchange resin removes anions, and finally the desired purity is achieved. A number of patents have been investigated for the combination of rectification and resin. For example, CN109160876A discloses a method for preparing electronic grade cyclohexanone, which comprises rectifying and adsorbing with ion exchange resin to obtain electronic grade cyclohexanone with ion content less than or equal to 10ppb and acidity less than or equal to 100 ppm. CN109251143A discloses a preparation method of electronic grade ethyl lactate, which comprises the steps of ion exchange resin adsorption, rectification and sub-boiling distillation, and the final product has ion content less than 1ppb and acidity less than 65 ppm. CN107098810A discloses a separation and purification method for preparing electronic-grade propylene glycol monomethyl ether acetate, which is to obtain electronic-grade propylene glycol monomethyl ether acetate with acidity less than 80ppm and content of each metal ion less than 1ppb by rectification and resin treatment. CN102898275A discloses a preparation method of high-purity isopropanol, which comprises the steps of molecular sieve dehydration, resin dehydration, reverse osmosis, high-temperature rectification, ion exchange and circulating filtration, wherein the steps are sequentially and continuously carried out for purification to obtain the high-purity isopropanol, and finally, the concentration of each single cation is less than 10ppt, and the concentration of each single anion is less than 1 ppb.
It has been found by the above patents that the anions are relatively difficult to remove. Undoubtedly, the method for effectively removing metal ions and anions by combined treatment is effective, but has the disadvantages of long steps, relatively complex operation and large amount of acid and alkali regeneration after resin failure, and is contrary to the green chemical concept advocated at present.
Disclosure of Invention
In order to solve the problem that the purity of the electronic grade reagent in the prior art is not high enough in the preparation process, in particular the problem that the content of metal ions and anion impurities is high or the removal process is complicated, the invention provides a preparation method of the electronic grade reagent, which comprises the following steps:
the method comprises the following steps of adding a raw material and a metal compound into a rectification system for rectification, wherein the rectification system is a conventional rectification device in the field, the structure of the rectification system is not particularly limited, and a plate-type rectification tower or a packing rectification tower and the like can be suitable for the application;
product collection is initiated after removal of the front component, which refers to all materials having a boiling point lower than that of the feedstock. If the boiling point of a certain substance is 120 ℃, all distilled components are front components before 120 ℃;
and detecting the content of metal ions and anions in the collected product to verify whether the purity of the product reaches the standard of the electronic grade reagent. Preferably, the mass concentration of the metal ions is measured by ICP-MS and the mass concentration of the anions is measured by IC. Preferably, the standard of the electronic grade reagent refers to the mass concentration of metal ions in the product being less than 1ppb and the mass concentration of anions being less than 10 ppb. According to the preparation method of the electronic grade reagent, the raw material containing impurities is purified to obtain the product, namely the electronic grade reagent.
Further, before the raw material to be prepared and the metal compound are added into a rectification equipment system for rectification, the method comprises the following steps: and cleaning the rectification system.
Further, wherein, wash rectification system, including the step:
the method comprises the following steps of cleaning a rectification system by using ultrapure water or acid ultrapure water solution, wherein the ultrapure water or acid ultrapure water solution means that before rectification, equipment needs to be cleaned to remove metal ions, anions and the like, and is generally cleaned by using the ultrapure water or acid ultrapure water solution, otherwise, unclean equipment can pollute products;
detecting the content of metal ions and anions in the receiving liquid in the rectification system;
and when the content of metal ions and anions in the receiving liquid of the rectification system is less than a specific threshold value, finishing cleaning the rectification system.
Further, the metal compound includes, but is not limited to, one or more of carbonate, bicarbonate, hydroxide compound and oxide of metal element.
Further, the metal compound includes, but is not limited to, metal compounds capable of forming a sparingly soluble salt with sulfate and chloride ions;
further, the carbonate includes one or more of sodium carbonate, potassium carbonate, calcium carbonate, copper carbonate, iron carbonate, basic copper carbonate, barium carbonate, silver carbonate, and lead carbonate.
Further, the bicarbonate includes, but is not limited to, one or more of sodium bicarbonate, potassium bicarbonate, calcium bicarbonate, and barium bicarbonate.
Further, the hydroxide compound includes, but is not limited to, one or more of sodium hydroxide, magnesium hydroxide, potassium hydroxide, calcium hydroxide, iron hydroxide, zinc hydroxide, barium hydroxide, silver hydroxide, and lead hydroxide.
Further, the oxide includes, but is not limited to, one or more of calcium oxide, magnesium oxide, iron oxide, copper oxide, barium oxide, silver oxide, and lead oxide.
Further, the ultra-pure water solution of the acid means that electronic grade acid is dissolved in ultra-pure water, and the acid includes but is not limited to hydrochloric acid, nitric acid and the like.
Further, when the content of metal ions and anions in the receiving liquid of the rectification system is less than a specific threshold value, the rectification system is cleaned, and the method comprises the following steps:
when the mass concentration of metal ions in the receiving liquid of the rectification system is less than 1ppb and the mass concentration of anions is less than 10ppb, the rectification system is cleaned. Ppm in the present invention means a mass concentration expressed in terms of parts per million of solute mass in the total solution mass, and is referred to as a ppm concentration; ppb refers to the mass concentration in a solution expressed as the parts per billion ratio of the mass of solute to the mass of the entire solution, and is referred to as the parts per billion concentration; ppt refers to mass concentration expressed in parts per trillion of solute mass to total solution mass, and is referred to as parts per trillion concentration.
Compared with the prior art, the invention has the advantages that:
the anions are difficult to remove relative to the metal ions because they can be distilled off as HCl along with the feedstock. The difficulty of separation is further increased if the starting material is somewhat basic and the anion can form a salt with it, such as the imidazole hydrochloride mentioned above. The method takes industrial-grade organic matters as raw materials, adds a proper amount of metal compounds during rectification, can further reduce metal ions and anions to ppb level, particularly effectively reduces the content of the anions in the electronic-grade reagent, obviously improves the purity of the electronic-grade reagent, and has simple steps and high purity.
Anions are volatilized out of the system in an acid form, a proper amount of metal compound is added during rectification, the anions can be neutralized with acid, the anions are fixed in a salt form, the anions and other raw materials are prevented from being rectified together, and the content of the metal ions in the product cannot be obviously improved. If the raw material to be purified is alkaline, a salt can be formed with anions, and the added metal compound can deprive the anions from the raw material, so that the volatilization of the anions is avoided. More preferably, the metal compound is a metal compound which forms a sparingly soluble salt with sulfate or chloride ions, such as barium hydroxide, calcium hydroxide, silver hydroxide, etc., and which further forms a sparingly soluble salt with anions, which can be removed at a lower dosage. The method has the advantages of simple purification process, high operability, high elasticity and wider application range.
Detailed Description
The advantages of the invention are explained in detail below with reference to specific embodiments.
It should be noted that the rectification equipment and the rectification process in the rectification system in the present application are not particularly limited, and can be implemented by using conventional rectification equipment and rectification parameters, such as a plate-type rectification column or a packed rectification column. The distillation equipment, distillation conditions, distillation parameters, and the like in the following examples are not intended to limit the method for purifying an electronic-grade reagent of the present application, but are merely exemplary for the purpose of facilitating understanding of the present invention and illustrating the technical effects of the method for purifying an electronic-grade reagent of the present invention.
Comparative example 1:
and (3) normal pressure rectification: 4Kg of technical grade isopropanol (raw material) is added into a rectifying tower for treatment, the height of the rectifying tower is 2.0m, the inner diameter of the rectifying tower is 50mm, and the used filler is preferably glass spring filler. Heating the bottom of the rectifying tower to the boiling point of the raw material, keeping the temperature of the tower at the boiling point of the raw material, condensing the discharged material by using water, collecting the material after the temperature reaches the boiling point of isopropanol, testing metal ions in the purified product by using ICP-MS (inductively coupled plasma-mass spectrometry), and testing anions by using IC (integrated circuit).
Example 1:
and (3) normal pressure rectification: 4Kg of technical grade isopropanol (raw material) and 20g of sodium hydroxide are added into a rectifying tower for treatment, the height of the rectifying tower is 2.0m, the inner diameter of the tower is 50mm, and the used filler is preferably glass spring filler. Heating the bottom of the rectifying tower to the boiling point of the raw material, keeping the temperature of the tower at the boiling point of the raw material, condensing the discharged material by using water, collecting the material after the temperature reaches the boiling point of isopropanol, testing metal ions in the purified product by using ICP-MS (inductively coupled plasma-mass spectrometry), and testing anions by using IC (integrated circuit).
Example 2:
and (3) normal pressure rectification: 4Kg of technical grade isopropanol (raw material) and 40g of sodium hydroxide are added into a rectifying tower for treatment, the height of the rectifying tower is 2.0m, the inner diameter of the tower is 50mm, and the used filler is preferably glass spring filler. Heating the bottom of the rectifying tower to the boiling point of the raw material, keeping the temperature of the tower at the boiling point of the raw material, condensing the discharged material by using water, collecting the material after the temperature reaches the boiling point of isopropanol, testing metal ions in the purified product by using ICP-MS (inductively coupled plasma-mass spectrometry), and testing anions by using IC (integrated circuit).
Example 3:
and (3) normal pressure rectification: 4Kg of industrial grade isopropanol (raw material) and 5g of calcium oxide were added to a rectifying tower for treatment, the height of the rectifying tower was 2.0m and the inner diameter of the tower was 50mm, and the used packing was preferably glass spring packing. Heating the bottom of the rectifying tower to the boiling point of the raw material, keeping the temperature of the tower at the boiling point of the raw material, condensing the discharged material by using water, collecting the material after the temperature reaches the boiling point of isopropanol, testing metal ions in the purified product by using ICP-MS (inductively coupled plasma-mass spectrometry), and testing anions by using IC (integrated circuit).
Example 4:
and (3) normal pressure rectification: 4Kg of industrial grade isopropanol (raw material), 2g of barium hydroxide and 2g of calcium hydroxide are added into a rectifying tower for treatment, the height of the rectifying tower is 2.0m, the inner diameter of the tower is 50mm, and the used filler is preferably glass spring filler. Heating the bottom of the rectifying tower to the boiling point of the raw material, keeping the temperature of the tower at the boiling point of the raw material, condensing the discharged material by using water, collecting the material after the temperature reaches the boiling point of isopropanol, testing metal ions in the purified product by using ICP-MS (inductively coupled plasma-mass spectrometry), and testing anions by using IC (integrated circuit).
Example 5:
and (3) normal pressure rectification: 4Kg of industrial-grade dimethyl sulfoxide (raw material), 3g of silver hydroxide and 2g of lead oxide are added into a rectifying tower for treatment, the height of the rectifying tower is 2.0m, the inner diameter of the tower is 50mm, and the used filler is preferably glass spring filler. Heating the bottom of the rectifying tower to the boiling point of the raw material, keeping the temperature of the tower at the boiling point of the raw material, condensing discharged materials by using water, collecting the materials after the boiling point of the dimethyl sulfoxide is reached, testing metal ions in the purified product by using ICP-MS (inductively coupled plasma-mass spectrometry), and testing anions by using IC (integrated circuit).
Example 6:
and (3) rectification under reduced pressure: 4Kg of industrial-grade benzotriazole (raw material), 1g of calcium oxide and 10g of magnesium hydroxide are added into a rectifying tower for treatment, the height of the rectifying tower is 2.0m, the inner diameter of the tower is 50mm, the negative pressure of the system is reduced to 2000Pa, and the used filler is preferably glass spring filler. Heating the bottom of the rectifying tower to the boiling point of the raw material, preserving the temperature of the tower at the boiling point of the raw material, condensing the discharged material by using water, collecting the material after the boiling point of the benzotriazole is reached, testing metal ions in the purified product by using ICP-MS (inductively coupled plasma-mass spectrometry), and testing anions by using IC (integrated circuit). It is worth noting that the rectification needs heating, and some compounds are unstable at high temperature and easy to decompose or oxidize, taking benzotriazole as an example, if decompression is not carried out, oxidative coupling can be carried out after heating, violent heat release can be caused, explosion can be caused, the boiling point is reduced after decompression, and the rectification can be carried out.
Example 7:
and (3) rectification under reduced pressure: 4Kg of industrial grade imidazole (raw material), 5g of copper oxide and 10g of iron oxide are added into a rectifying tower for treatment, the height of the rectifying tower is 2.0m, the inner diameter of the tower is 50mm, the negative pressure of the system is reduced to 2000Pa, and the used filler is preferably glass spring filler. Heating the bottom of the rectifying tower to the boiling point of the raw material, preserving the temperature of the tower at the boiling point of the raw material, condensing the discharged material by using water, collecting the material after the boiling point of imidazole is reached, testing metal ions in the purified product by using ICP-MS (inductively coupled plasma-mass spectrometry), and testing anions by using IC (integrated circuit).
TABLE 1 ICP-MS test results and IC test results before and after purification of various raw materials in comparative example 1 and examples 1-7
As can be seen from the test results in table 1, by comparative example 1, we found that the rectification process without adding metal oxide can remove metal ions, but anions are difficult to reduce to ppb level ("ppb level", i.e., "< DL", i.e., "< 0.01 ppm" or "< 10 ppb" in the IC test results in table 1), whereas the metal compounds are added during the rectification process in examples 1 to 7 per se, so that the contents of metal ions and anions in the purified product are significantly reduced, for example, the content of metal ions is <1ppb, and the content of anions is <10 ppb.
Examples 1-4 were the same as the raw material of comparative example 1 and the ICP-MS test results (ppb) of the metal ions and the IC test results (ppm) of the anions were the same, as shown in example 1, the raw material (4Kg of technical grade isopropanol) and 20g of sodium hydroxide were simultaneously added to the rectification column for rectification, the sodium hydroxide fixed the anions in the form of salts, the anion concentration in the product was greatly reduced, and the anion content after purification was all < DL.
In example 2, the raw material (4Kg of technical grade isopropanol) and 40g of sodium hydroxide were simultaneously fed into the rectifying column to remove anions, and the content of sodium ions in the product was not increased but decreased to 0.29ppb (0.41 ppb after purification in example 1) relative to the content of sodium ions after purification in example 1, which indicates that sodium ions were not distilled off together with the raw material.
In example 3, the raw material (4Kg of technical grade isopropanol) and 5g of calcium oxide, which form insoluble salts with sulfate and chloride ions, were added simultaneously to the rectification column, and a better purification effect was obtained at a lower addition.
In examples 4 to 7, the composition of the raw material and the metal compound is added to the rectification column during the rectification process, which not only serves to remove the metal ions in the raw material, but also serves to remove the anions in the raw material with high efficiency, indicating that the addition of the metal compound or the composition thereof during the rectification process is an effective method for removing the anions.
In conclusion, compared with a method for removing anions in raw materials by combining rectification and resin in the prior art, the method for preparing the electronic-grade reagent does not need a mode of combining ion exchange resin and a rectification system in the prior art, metal ions and anions in the raw materials can be efficiently removed by adding a metal compound in the rectification process, and the electronic-grade reagent is simple in preparation process, high in product purity, high in operability, high in elasticity and wide in application range.
The embodiments of the present invention have been described in detail, but the embodiments are merely examples, and the present invention is not limited to the embodiments described above. Any equivalent modifications and substitutions to those skilled in the art are also within the scope of the present invention. Accordingly, equivalent changes and modifications made without departing from the spirit and scope of the present invention should be covered by the present invention.
Claims (13)
1. A method of preparing an electronic grade reagent comprising the steps of:
adding the raw materials and metal compounds into a rectification system for rectification;
collecting the product after removing the former component;
and detecting the content of metal ions and anions in the collected product to verify whether the purity of the product reaches the standard of the electronic grade reagent.
2. The method for preparing an electronic grade reagent according to claim 1, wherein before the raw material to be prepared and the metal compound are fed into a rectification equipment system for rectification, the method comprises the following steps: and cleaning the rectification system.
3. The method of claim 2, wherein cleaning the rectification system comprises the steps of: cleaning the rectification system by adopting ultrapure water or acid ultrapure water solution;
detecting the content of metal ions and anions in the rectification system;
and when the content of the metal ions and the anions in the rectification system is less than a specific threshold value, finishing cleaning the rectification system.
4. The method of claim 1, wherein the metal compound comprises one or more of a carbonate, a bicarbonate, a hydroxide, and an oxide of a metal element.
5. The process for preparing an electronic grade reagent according to claim 4, wherein the metal compound is a metal compound capable of forming a sparingly soluble salt with sulfate or chloride ions.
6. The method of claim 4, wherein the carbonate comprises one or more of sodium carbonate, potassium carbonate, calcium carbonate, copper carbonate, iron carbonate, basic copper carbonate, barium carbonate, silver carbonate, and lead carbonate.
7. A method of preparing an electronic grade reagent according to claim 4 wherein the bicarbonate comprises one or more of sodium bicarbonate, potassium bicarbonate, calcium bicarbonate, barium bicarbonate.
8. The method of claim 4, wherein the hydroxide compound comprises one or more of sodium hydroxide, magnesium hydroxide, potassium hydroxide, calcium hydroxide, ferric hydroxide, zinc hydroxide, barium hydroxide, silver hydroxide, and lead hydroxide.
9. The method of claim 4, wherein the oxide comprises one or more of calcium oxide, magnesium oxide, iron oxide, copper oxide, barium oxide, silver oxide, and lead oxide.
10. A process for the preparation of an electronic grade reagent according to claim 1 or 3 wherein the mass concentration of metal ions is measured by ICP-MS and the mass concentration of anions is measured by IC.
11. The method of claim 1, wherein the standard of the electronic grade reagent is a product with a mass concentration of metal ions <1ppb and anion <10 ppb.
12. The method of preparing an electronic grade reagent of claim 3 wherein the ultra pure aqueous solution of the acid is an electronic grade acid dissolved in ultra pure water, the acid comprising hydrochloric acid and/or nitric acid.
13. The method for preparing an electronic grade reagent according to claim 3, wherein when the content of metal ions and anions in the rectification system is less than a specific threshold, the rectification system is cleaned, and the method comprises the following steps:
when the mass concentration of metal ions in the rectification system is less than 1ppb and the mass concentration of anions in the rectification system is less than 10ppb, the washing of the rectification system is ended.
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| CN114644348A (en) * | 2022-03-18 | 2022-06-21 | 西安吉利电子新材料股份有限公司 | Preparation system and method for directly producing electronic-grade ammonia water from ammonia gas |
| CN114989005A (en) * | 2022-05-30 | 2022-09-02 | 湖北兴福电子材料有限公司 | Preparation method of electronic grade acetic acid |
| CN115028147A (en) * | 2022-06-30 | 2022-09-09 | 江苏淮河化工有限公司 | Process for continuously preparing electronic-grade nitric acid by rectification and stripping integrated method |
| CN115181019A (en) * | 2022-08-26 | 2022-10-14 | 东华工程科技股份有限公司 | Process for preparing electronic grade glycolic acid solution by hydrolyzing methyl glycolate |
| CN115353121A (en) * | 2022-09-01 | 2022-11-18 | 阜新泽程化工有限责任公司 | Industrial production method of electronic pure ammonium sulfite |
| CN115784952A (en) * | 2022-10-09 | 2023-03-14 | 新疆兴发化工有限公司 | Purification process of electronic grade dimethyl sulfoxide |
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